CN100571900C - A kind of cleaning method of anode oxidize spare parts surface - Google Patents
A kind of cleaning method of anode oxidize spare parts surface Download PDFInfo
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- CN100571900C CN100571900C CNB2006101655595A CN200610165559A CN100571900C CN 100571900 C CN100571900 C CN 100571900C CN B2006101655595 A CNB2006101655595 A CN B2006101655595A CN 200610165559 A CN200610165559 A CN 200610165559A CN 100571900 C CN100571900 C CN 100571900C
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Abstract
The cleaning method of anode oxidize spare parts surface of the present invention, mainly comprise with an organic solvent, the method for acid solution, oxidant fluorinated ketone and the ultrasonic cleaning of alkaline solution, dilution removes the complicated pollutant on chamber anodized surface, can remove greasy dirt, metal, slaine respectively, contain the complicated accessory substance of F; This cleaning method is a kind of not damaged, the effective ways of anode purge oxidized surface fast and effectively, if it also is that the cleaning method of employing this patent of very trace cleans the anodized surface of polycrystal etching machine chamber that damage is arranged, can reach the complicated pollutant on not damaged, simple and effective removal surface, and make chamber return to normal state, meet manufacturing technique requirent, this patent also can be used for having the cleaning of the parts of anodized surface.
Description
Technical field
The present invention relates to a kind of cleaning method of object, relate in particular to the cleaning method of the anode oxidize spare parts surface in the microelectronic technique process ionic medium cavity.
Background technology
Along with the development of the technology of semiconductor chips, technology node develops into 65nm from 250nm, even below the 45nm, the size of silicon chip also is increased to 300mm from 200mm, and under these circumstances, the cost of every silicon chip becomes more and more higher.Technological requirement to the processing silicon chip is more and more stricter.Semi-conductive processing need be passed through multiple working procedure, comprises deposition, photoetching, etching, side wall etc., and etching technics is wherein comparatively complicated one, and the state of plasma etch process ionic medium body, every parameters of technique process etc. are directly related with the etching result.
In polycrystalline silicon semiconductor dry etch process process,, can produce a lot of complicated component accessory substances along with carrying out corresponsively.Clean though after each technology, carry out dry method, promptly adopt sulfur hexafluoride SF6 or oxygen O
2Plasma gas Deng gas is removed accessory substance in the chamber or pollutant under certain vacuum and radio-frequency power, most of this class accessory substance can be discharged reative cell by molecular pump and dried pump with containing the SF6 plasma reaction, but the accessory substance that also has fraction is attached on the reaction chamber wall.Accessory substance is in the process environments of reative cell, a series of division polymerisation can take place, reconfigure polymer for the constituent structure complexity, the accessory substance of this moment has been difficult to remove with the method that dry method is cleaned, this polymer film that is attached to constituent structure complexity on the inwall can constantly be accumulated along with proceeding of technology, and this layer film stability is not strong, at any time can split away off from inwall and pollute silicon chip, so need the chamber that reative cell inside is exposed to process environments regularly be cleaned.
Common cleaning means are to adopt organic solvent such as ethanol, isopropyl alcohol etc., NH
4OH or KOH alkaline solution, HCl, HNO
3Can effectively remove the organic and metal pollutant on its surface to a certain extent Deng acid solution, but for the pollutant that contains F such as A1F3, Al-Si-F-etc., this type of pollutant reaction activity is low, common cleaning agent poor effect
Summary of the invention
The cleaning method that the purpose of this invention is to provide a kind of anode oxidize spare parts surface can be realized the wet-cleaning of carrying out of antianode oxidation part surface, and is little to the piece surface damage, and satisfies instructions for use fully.When the etching machine carries out normal process such as polycrystal etching, after polycrystal etching technology,, recover the normal process conditions of chamber, thereby satisfy production requirement for the accessory substance in the chamber provides quick, easy, effectively removes method.
The objective of the invention is to be achieved through the following technical solutions:
1, a kind of cleaning method of anode oxidize spare parts surface may further comprise the steps:
A, usefulness organic solvent cleaning components surface;
B, usefulness alkaline solution cleaning components surface;
C, usefulness acid solution cleaning components surface;
D, with the mixed solution cleaning components surface of fluorinated ketone or fluorinated ketone and organic solvent;
E, use the ultrasonic wave cleaning components.
Also comprise before the described steps A:
With ultra-pure water cleaning components surface; Specifically spray the spray time that piece surface is no less than setting, dry up the surface of part with clean gases at high pressure with ultra-pure water.
Described steps A comprises:
A1, use the organic solvent wiper element, come off until the impurity that does not have the band look; And/or,
A2, the spray time of setting with organic solvent spray part, and can repeat repeatedly, and each spray time and used organic solvent can be identical or different; And/or,
A3, soak the soak time that part is set, and can repeat repeatedly with organic solvent, and each soak time and used organic solvent can be identical or different;
And/or,
A4, in wiping, spray and/or soak and also comprise after part cleans and wash piece surface with ultra-pure water, and dry up the surface of part with the gases at high pressure of cleaning.
Described organic solvent is:
Content is 100% isopropyl alcohol; Perhaps,
Content is 100% ethanol; Perhaps,
Content is 100% acetone;
Described isopropyl alcohol, ethanol and acetone are not less than the primary standard of SEMI standard.
Described step B comprises:
B1, soak the scavenging period that part is no less than setting with alkaline solution;
B2, wash piece surface with ultra-pure water again, and dry up the surface of part with the gases at high pressure of cleaning with clean cleaning piece wiper element.
Described alkaline solution comprises: ammonium hydroxide NH
4OH, oxydol H
2O
2With water H
2O, the mass content ratio of its each component is:
NH
4OH: H
2O
2: H
2O, ratio is 1: 1: 1～20.
Described step C comprises:
C1, use the acid solution wiper element, be no more than the wiping time of setting;
C2, wash piece surface, and dry up the surface of part with clean gases at high pressure with ultra-pure water.
8, the cleaning method of anode oxidize spare parts surface according to claim 7 is characterized in that:
Described acid solution comprises nitric acid HNO
3, hydrofluoric acid HF, ammonium persulfate (NH
4)
2SO
4With water H
2O, the mass content ratio of its each component is:
HNO
3: HF: (NH
4)
2SO
4: H
2O is 1: 1: 1: 10～50.
Described step D comprises:
With mass content is that the fluorinated ketone of 1%-20% and the mixed solution of organic solvent soak piece surface, washes piece surface with ultra-pure water again, and dries up the surface of part with clean gases at high pressure.
Described step e comprises:
E1, the ultrasonic tank of part being put into ultra-pure water were cleaned 20-40 minute with the 10-26KHz frequency, and the ultra-pure water water temperature is 40-70 ℃, and ultrasonic energy density is less than 30 watts/gallon; And/or,
E2, part is put into deionized water ultrasonic tank to clean 20-30 minute than the 30-45KHz frequency, the deionized water water temperature is 40-70 ℃, ultrasonic energy density is less than 30 watts/gallon.
As seen from the above technical solution provided by the invention, the cleaning method of anode oxidize spare parts surface of the present invention, mainly comprise with an organic solvent, the method for acid solution, fluorinated ketone solution and the ultrasonic cleaning of alkaline solution, dilution removes the complicated pollutant on chamber anodized surface, can remove greasy dirt, metal, slaine respectively, contain the complicated accessory substance of F; This cleaning method is a kind of not damaged, the effective ways of anode purge oxidized surface fast and effectively, if it also is that the cleaning method of employing this patent of very trace cleans the anodized surface of polycrystal etching machine chamber that damage is arranged, can reach the complicated pollutant on not damaged, simple and effective removal surface, and make chamber return to normal state, meet manufacturing technique requirent, this patent also can be used for having the cleaning of the parts of anodized surface.
The specific embodiment
The cleaning method of anode oxidize spare parts surface of the present invention, mainly comprise with an organic solvent, the method for acid solution, fluorinated ketone solution and the ultrasonic cleaning of alkaline solution, dilution removes the complicated pollutant on chamber anodized surface, can remove greasy dirt, metal, slaine respectively, contain the complicated accessory substance of F; This cleaning method is a kind of not damaged, the effective ways of anode purge oxidized surface fast and effectively, also is trace very if damage is arranged.
Use and of the present inventionly may further comprise the steps generally:
One, with organic solvent cleaning components surface;
The purpose of this process is to remove the organic impurities of reaction chamber anodized surface.
The method of cleaning has three kinds, can use simultaneously, also can use separately.
1, uses the organic solvent wiper element, come off until the impurity that does not have the band look;
Available non-dust cloth (clean cleaning piece) dips in the organic solvent wiper element, does not have color until non-dust cloth.
2, soak the soak time that part is set with organic solvent, use clean cleaning piece wiper element again, and can repeat repeatedly, come off until the impurity that does not have the band look.
Available organic solvent soaks the soak time that part is no less than setting, uses the non-dust cloth wiper element again, does not have color until non-dust cloth.In order to reach the requirement of cleaning, can repeat repeatedly to soak and wiping.
3, the spray time of setting with organic solvent spray part is used clean cleaning piece wiper element again, and can be repeated repeatedly, comes off until the impurity that does not have the band look.
Available organic solvent spray part is no less than the spray time of setting, uses the non-dust cloth wiper element again, does not have color until non-dust cloth.In order to reach the requirement of cleaning, can repeat repeatedly to spray and wiping.
With after organic solvent wiping and/or the soaking and washing, the washing time of setting with ultra-pure water (resistance greater than 18 Ω/cm, 25 ℃) flushing piece surface, and dry up the surface of part with the gases at high pressure (using nitrogen usually) of cleaning.
The organic solvent here is:
Isopropyl alcohol, ethanol or acetone,
Simultaneously, before cleaning,, and, come off until the impurity that does not have the band look with clean cleaning piece wiper element with the washing time of ultra-pure water flushing piece surface setting with organic solvent; And dry up the surface of part with clean gases at high pressure (using nitrogen usually).
Two, with alkaline solution cleaning components surface;
The purpose of this process is organic impurities, metal impurities and the fluoride of removing in the deposit of reaction chamber anodized surface.
Soak the scavenging period that part is no less than setting with alkaline solution; Use the non-dust cloth wiper element then, do not have color until non-dust cloth.Wash piece surface with ultra-pure water again, and dry up the surface of part with clean gases at high pressure.
The prescription of described alkaline solution comprises ammonium hydroxide NH
4OH, oxydol H
2O
2With water H
2O, the mass content ratio of its each component is:
NH
4OH: H
2O
2: H
2O is 1～5: 1～10: 1-20; Preferred content ratio is:
NH
4OH: H
2O
2: H
2O is 1～3: 1～5: 1～15; Its optimum content ratio is:
NH
4OH: H
2O
2: H
2O is 1: 1: 10.
Three, with acid solution cleaning components surface
This process purpose is metal impurities and the electrode impurities of removing in the deposit of reaction chamber anodized surface.
Use the acid solution wiper element, be no more than the wiping time of setting, and in time use the pure water rinsing piece surface.And dry up the surface of part with clean gases at high pressure.
The prescription of described acid solution comprises nitric acid HNO
3, hydrofluoric acid HF, ammonium persulfate (NH
4)
2SO
4With water H
2O, the mass content ratio of its each component is:
HNO
3: HF: (NH
4)
2SO
4: H
2O is 1～5: 1～10: 1～5: 1-50; Preferred content ratio is:
HNO
3: HF: (NH
4)
2SO
4: H
2O is 1～3: 1～5: 1～3: 1～20; Its optimum content ratio is:
HNO
3: HF: (NH
4)
2SO
4: H
2O is; 1: 1: 1: 10.
The effect of ammonium persulfate is to prevent from HF and silicon grain and contain the fluosilicic acid (H2SiF6) that the impurity reaction of Si generates to be bonded in anodized surface.
Four, with fluorinated ketone solution cleaning components surface
This process purpose is the fluorine-containing material of removing in the deposit of reaction chamber anodized surface.
With mass content is that the fluorinated ketone of 1%-20% and the mixed solution of organic solvent soak piece surface, washes piece surface with ultra-pure water again, and dries up the surface of part with clean gases at high pressure.
Five, part is put into ultrasonic tank, clean the time of setting.
This process purpose is some remaining metallic particles of removing in the deposit of reaction chamber anodized surface.
Usually can be divided into low frequency and clean with high frequency and clean, it is that ultrasonic tank with part is put into ultra-pure water was cleaned 20-40 minute with the 10-26KHz frequency that low frequency cleans, and the ultra-pure water water temperature is 40-70 ℃, and ultrasonic energy density is less than 30 watts/gallon; High frequency clean be part is put into deionized water ultrasonic tank to clean 20-30 minute than the 30-45KHz frequency, the deionized water water temperature is 40-70 ℃, ultrasonic energy density is less than 30 watts/gallon.
At last, wash the washing time that piece surface is set, and dry up the surface of part with clean gases at high pressure with ultra-pure water; Again with cleaning piece wiper element or oven dry part with cleaning.
Preferred embodiment of the present invention is:
Step 1, at room temperature use the ultra-pure water (spray of resistance 〉=18 Ω/cm) anodic oxide coating piece surface at least 5 minutes, can remove the lower particulate pollutant of some adsorptivities of surface, dry up the surface of part then with clean gases at high pressure, the general available N that has filter (0.05-0.1 μ m)
2Rifle dries up the surface.
Step 2, use electron level isopropyl alcohol remove the organic impurities of chamber anodized surface, also can use as ethanol, acetone etc. if other organic solvent meets the requirements, but prerequisite are to cause the pollution once more of anodic oxidation part; Again with ultra-pure water flushing, dry up the surface of part, the generally available N that has filter (0.05-0.1 μ m) with clean gases at high pressure
2Rifle dries up the surface.
Step 3, use have oxidisability weakly alkaline solution NH
4OH: H
2O
2: H
2O (1: 1: 1-1: 1: 20) soaks the anodized surface of chamber, at least 30 minutes, can be according to actual conditions time expands, and wash with ultra-pure water again with the non-dust cloth wiping, and dry up the surface of part, the general available N that has filter (0.05-0.1 μ m) with clean gases at high pressure
2Rifle dries up the surface.H
2O
2Be a kind of strong oxidizer, both can become solable matter or gas to oxidation operation, also can be oxidized to metal impurities the metal ion of high price, and metal ion can form with ammoniacal liquor and Dings De Network than Wen and close ion, thereby be removed.This kind alkaline solution can be removed organic impurities, metal impurities and fluoride.
Step 4, use acid solution HNO
3: HF: H
2O (1: 1: 10-1: 1: 50), and contain an amount of ammonium persulfate such as 1wt%-3wt% comes the wash chamber anodized surface, avoid the corrosion of acid solution antianode oxidized surface, the non-dust cloth that employing speckles with this acid liquid carries out wiping, and wash with ultra-pure water at once, wash with ultra-pure water again after the cleaning, and also dry up the surface of part, the general available N that has filter (0.05-0.1 μ m) with clean gases at high pressure
2Rifle dries up the surface.HNO3 in this acid solution can remove metallic particles and electrode impurities, for example: HNO
3+ Cu=Cu (NO
3)
2+ H
2, HF can remove silicon grain and contain the impurity of Si, and wherein the effect of ammonium persulfate is the fluosilicic acid (H that prevents HF and silicon grain and contain the impurity reaction generation of Si
2SiF
6) be bonded in anodized surface, for example HF and SiO
2React as follows:
4HF+SiO
2＝SiF
4+2H
2O
6HF+SiO
2＝H
2SiF
6+2H
2O
Step 5, about 80 ℃, use fluorinated ketone 1-20wt% solution to soak the chamber anodized surface,, and and dry up the surface of part, the generally available N that has filter (0.05-0.1 μ m) with clean gases at high pressure again with the ultra-pure water flushing
2Rifle dries up the surface; Fluorinated ketone 1wt%-20wt% solution can be removed complicated things such as containing F as-C-Al-F-, under heated state, improves the activity and the dissolubility of pollutant and fluorinated ketone solution simultaneously, and fluorinated ketone has heat endurance preferably, and boiling point is more than 150 ℃.
Step 6, put into ultrasonic tank and carry out oarse-grained removal with lower frequency (10-26KHz), ultrasonic 20-40 minute, the ultra-pure water water temperature was 40-70 ℃, and ultrasonic energy density is lined with non-dust cloth to prevent the water seal less than 30 watts/gallon between part and the supporting plate.Time is not long, in order to avoid the infringement surface.
Part is put into ultrasonic tank and is carried out fine purifiation with upper frequency (30-45KHz), and ultrasonic 20-30 minute, 18,000,000 deionized water water temperatures were 40-70 ℃, and ultrasonic energy density is lined with non-dust cloth to prevent the water seal less than 30 watts/gallon between part and the supporting plate.Time is not long, in order to avoid the infringement surface.
Step 7, ultra-pure water spray ceramic component surface, and also dry up the surface of part with clean gases at high pressure, the general available N that has filter (0.05-0.1 μ m)
2Rifle dries up the surface, uses the non-dust cloth wiping.Also to dry 80～120 ℃ of temperature, 1.5～2.5 hours to part
After cleaning with the method, the pollutant of piece surface is removed fully, and anode oxidize spare parts surface recovers cleaning, utilizes the surface particles detector to detect, and piece surface particle situation conforms to quality requirements; Simultaneously, use surfagauge to test, it is little that Part Surface Roughness is cleaned the front and back variation, shows that the cleaning damage is less.Part after the cleaning satisfies the requirement of normal process fully, reaches cleaning performance.
As seen, adopt the cleaning method of this patent that the anodized surface of polycrystal etching machine chamber is cleaned, can reach the complicated pollutant on not damaged, simple and effective removal surface, and make chamber return to normal state, meet manufacturing technique requirent, this patent also can be used for having the cleaning of the parts of anodized surface.
In addition, the chemical liquids that is used in the cleaning method must meet the semicon industry standard, and its grade is minimum to be 1 grade.
The above; only for the preferable specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, and anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.
Claims (9)
1, a kind of cleaning method of anode oxidize spare parts surface is characterized in that, may further comprise the steps:
A, usefulness organic solvent cleaning components surface;
B, usefulness alkaline solution cleaning components surface, described alkaline solution comprises: ammonium hydroxide NH
4OH, oxydol H
2O
2With water H
2O, the mass content ratio of its each component is: NH
4OH: H
2O
2: H
2O, ratio is 1: 1: 1～20;
C, usefulness acid solution cleaning components surface;
D, with the mixed solution cleaning components surface of fluorinated ketone or fluorinated ketone and organic solvent;
E, use the ultrasonic wave cleaning components.
2, the cleaning method of anode oxidize spare parts surface according to claim 1 is characterized in that, also comprises before the described steps A:
With ultra-pure water cleaning components surface; Specifically spray the spray time that piece surface is no less than setting, dry up the surface of part with clean gases at high pressure with ultra-pure water.
3, the cleaning method of anode oxidize spare parts surface according to claim 1 is characterized in that, described steps A comprises the one or more steps among the following A1 to A3:
A1, use the organic solvent wiper element, come off until the impurity that does not have the band look;
A2, the spray time of setting with organic solvent spray part, and can repeat repeatedly, and each spray time and used organic solvent can be identical or different;
A3, soak the soak time that part is set, and can repeat repeatedly, and each soak time and used organic solvent can be identical or different with organic solvent;
After wiping, spray and/or immersion part clean, also comprise and wash piece surface, and dry up the surface of part with clean gases at high pressure with ultra-pure water.
According to the cleaning method of claim 1 or 3 described anode oxidize spare parts surfaces, it is characterized in that 4, described organic solvent is:
Content is 100% isopropyl alcohol; Perhaps,
Content is 100% ethanol; Perhaps,
Content is 100% acetone;
Described isopropyl alcohol, ethanol and acetone are not less than the primary standard of SEMI standard.
5, the cleaning method of anode oxidize spare parts surface according to claim 1 and 2 is characterized in that, described step B comprises:
B1, soak the scavenging period that part is no less than setting with alkaline solution;
B2, wash piece surface with ultra-pure water again, and dry up the surface of part with the gases at high pressure of cleaning with clean cleaning piece wiper element.
6, the cleaning method of anode oxidize spare parts surface according to claim 1 and 2 is characterized in that, described step C comprises:
C1, use the acid solution wiper element, be no more than the wiping time of setting;
C2, wash piece surface, and dry up the surface of part with clean gases at high pressure with ultra-pure water.
7, the cleaning method of anode oxidize spare parts surface according to claim 6 is characterized in that:
Described acid solution comprises nitric acid HNO
3, hydrofluoric acid HF, ammonium persulfate (NH
4)
2SO
4With water H
2O, the mass content ratio of its each component is:
HNO
3: HF: (NH
4)
2SO
4: H
2O is 1: 1: 1: 10～50.
8, the cleaning method of anode oxidize spare parts surface according to claim 1 and 2 is characterized in that, described step D comprises:
With mass content is that the fluorinated ketone of 1%-20% and the mixed solution of organic solvent soak piece surface, washes piece surface with ultra-pure water again, and dries up the surface of part with clean gases at high pressure.
9, the cleaning method of anode oxidize spare parts surface according to claim 1 and 2 is characterized in that, described step e comprises:
E1, the ultrasonic tank of part being put into ultra-pure water were cleaned 20-40 minute with the 10-26KHz frequency, and the ultra-pure water water temperature is 40-70 ℃, and ultrasonic energy density is less than 30 watts/gallon; And/or,
E2, the ultrasonic tank of part being put into deionized water were cleaned 20-30 minute with the 30-45KHz frequency, and the deionized water water temperature is 40-70 ℃, and ultrasonic energy density is less than 30 watts/gallon.
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| CNB2006101655595A CN100571900C (en) | 2006-12-21 | 2006-12-21 | A kind of cleaning method of anode oxidize spare parts surface |
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|---|---|---|---|
| CNB2006101655595A CN100571900C (en) | 2006-12-21 | 2006-12-21 | A kind of cleaning method of anode oxidize spare parts surface |
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| CN100571900C true CN100571900C (en) | 2009-12-23 |
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| CN103372554A (en) * | 2012-04-13 | 2013-10-30 | 于强 | Pressurizer fixed sleeve shaft seal cleaning process |
| CN102671890A (en) * | 2012-04-28 | 2012-09-19 | 鞍山市联达电子有限公司 | Chemical cleaning method for silicon-controlled rectifier chips |
| CN104998857A (en) * | 2014-04-15 | 2015-10-28 | 宁波宝新不锈钢有限公司 | Dipping repair method of slide way of ABB shape meter slide ring |
| CN103986044B (en) * | 2014-05-22 | 2016-03-30 | 西安空间无线电技术研究所 | A kind of surface treatment method of inner conductor of radio frequency coaxial connector |
| CN104195575A (en) * | 2014-08-27 | 2014-12-10 | 富乐德科技发展（天津）有限公司 | Cleaning method for removing TiN and Ti films attached to surface of metal part |
| CN105470103B (en) * | 2014-09-09 | 2019-02-05 | 南京理工大学 | High-performance AlGaN photocathode chemical cleaning method |
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| CN111804674A (en) * | 2020-04-27 | 2020-10-23 | 安徽富乐德科技发展股份有限公司 | Method for cleaning pollutants on surface of anode oxidation part in ETCH (electronic toll Collection) equipment |
| CN112678759B (en) * | 2020-12-31 | 2023-08-01 | 浙江凯圣氟化学有限公司 | Method for cleaning ultrapure hydrofluoric acid package |
| CN114456884A (en) * | 2021-12-30 | 2022-05-10 | 安莱博医药(苏州)有限公司 | ICP component cleaning agent |
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Address after: 100176 Beijing economic and Technological Development Zone, Wenchang Road, No. 8, No. Patentee after: Beijing North China microelectronics equipment Co Ltd Address before: 100016, building 2, block M5, No. 1 East Jiuxianqiao Road, Beijing, Chaoyang District Patentee before: Beifang Microelectronic Base Equipment Proces Research Center Co., Ltd., Beijing |
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